Acetate fiber textile jean fabric and preparation process thereof

Abstract

The application relates to the technical field of textile fabrics, in particular to an acetate fiber textile jean fabric and a preparation process thereof. The preparation process comprises the following steps: step S1: mixing acetate fiber, cool fiber and cotton fiber to obtain warp yarn; step S2: mixing cool fiber, cotton fiber and bamboo fiber to obtain weft yarn; and step S3: weaving the warp yarn and the weft yarn to obtain a gray fabric, and then carrying out gray fabric turning, singeing, desizing, tentering and pre-shrinking and setting on the gray fabric to obtain a jean fabric. The jean fabric prepared by the application has excellent antibacterial performance, excellent cool performance, durability and comfort, so that the service life of the jean fabric is prolonged.

Description

Technical Field

[0001] This invention relates to the field of textile fabric technology, specifically to an acetate fiber denim fabric and its preparation process. Background Technology

[0002] With increasing emphasis on environmental protection and sustainable development, cellulose acetate, as a fiber material with excellent biodegradability, has received growing attention. Cellulose acetate possesses excellent moisture absorption and breathability, a soft and comfortable feel, and good abrasion resistance, thus it is widely used in the textile industry.

[0003] However, existing technologies present several challenges in preparing denim fabrics from cellulose acetate. First, denim fabrics typically require high strength and abrasion resistance, but cellulose acetate exhibits relatively low strength and abrasion resistance, failing to meet these requirements. Second, cellulose acetate has limited antibacterial properties; these properties gradually weaken or even disappear completely with prolonged use and repeated washing. Furthermore, the cooling effect of cellulose acetate is significantly reduced in hot and humid environments.

[0004] Therefore, we propose a denim fabric made of acetate fiber and its preparation process. Summary of the Invention

[0005] The purpose of this invention is to provide an acetate fiber denim fabric and its preparation process to solve the problems mentioned in the background art.

[0006] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0007] A process for preparing acetate fiber denim fabric includes the following steps:

[0008] Step S1: Blend cellulose acetate, cooling fiber and cotton fiber to obtain warp yarn;

[0009] Step S2: Blend the cooling fiber, cotton fiber and bamboo fiber to obtain the weft yarn;

[0010] Step S3: Weave the warp and weft yarns to obtain the greige fabric. Then, sequentially perform greige fabric turning, singeing, desizing, stretching, and pre-shrinking to obtain the denim fabric.

[0011] Furthermore, the mass ratio of the acetate fiber, the cooling fiber, and the cotton fiber is 1:(1-2):(2-3).

[0012] Furthermore, the mass ratio of the cooling fiber, cotton fiber, and bamboo fiber is 1:(2-3):(0.5-1.0).

[0013] Furthermore, the diameter of the warp yarn is 48-51 μm, the diameter of the weft yarn is 42-45 μm, the warp yarn density is 70-79 yarns / cm, and the weft yarn density is 40-50 yarns / cm.

[0014] Furthermore, the method for preparing the cellulose acetate is as follows:

[0015] Step (1): Under nitrogen protection, cellulose acetate, N,N-dimethylacetamide, and triethylamine are mixed evenly, the system temperature is adjusted to -10 to -5℃, and a mixed solution of methacryloyl chloride and N,N-dimethylacetamide is added dropwise over 1 to 2 hours. The temperature is then raised to 20 to 30℃ and the reaction is carried out for 22 to 24 hours. After filtration, washing, and drying, cellulose acetate containing double bonds is obtained.

[0016] Step (2): Mix 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 2-chloro-4,6-dimethoxy-1,3,5-triazine and anhydrous N,N-dimethylformamide evenly, react in an ice bath for 1-2 hours, adjust the pH of the system to 7.3-7.5, add methacrylamide and mix evenly, react in an ice bath for 3-5 hours, and obtain the antibacterial agent after rotary evaporation;

[0017] Step (3): Under nitrogen protection, mix cellulose acetate containing double bonds, antibacterial agent and deionized water evenly, heat to 70-80℃, add potassium persulfate and deionized water solution dropwise over 1-2 hours, react for 6-8 hours, filter, wash and dry to obtain modified cellulose acetate;

[0018] Step (4): Mix the modified cellulose acetate and dichloromethane evenly, and use dry spinning method to obtain cellulose acetate.

[0019] Furthermore, in step (1), the mass ratio of cellulose acetate to N,N-dimethylacetamide, triethylamine, and methacryloyl chloride is 1:(12-15):(0.8-1.0):(0.8-1.0), and the mass ratio of methacryloyl chloride to N,N-dimethylacetamide is 1:(6-8).

[0020] Furthermore, in step (2), the mass ratio of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 2-chloro-4,6-dimethoxy-1,3,5-triazine, and anhydrous N,N-dimethylformamide is 1:(0.8-1.0):(5-7), and the mass of methacrylamide is 40-50% of the mass of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid.

[0021] Furthermore, in step (3), the mass ratio of double-bonded cellulose acetate, antibacterial agent and deionized water is 1:(1.0-1.5):(4-6); the mass of potassium persulfate is 3-5% of the mass of double-bonded cellulose acetate, and the mass ratio of potassium persulfate and deionized water is 1:(300-400).

[0022] Furthermore, in step (4), the mass ratio of modified cellulose acetate to dichloromethane is 1:(2-4).

[0023] In the above technical solution, cellulose acetate containing double bonds is prepared by reacting cellulose acetate with methacryloyl chloride. Simultaneously, an antibacterial agent containing double bonds is obtained through an amidation reaction of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid and methacrylamide. Finally, under the action of an initiator, the double bonds in the cellulose acetate containing double bonds are reacted with the double bonds in the antibacterial agent to obtain modified cellulose acetate. This allows the antibacterial agent to firmly adhere to the surface of cellulose, enhancing the antibacterial effect and improving the antibacterial properties of cellulose.

[0024] Furthermore, the method for preparing the cooling fiber is as follows:

[0025] Step 1: Mix spandex slices and sodium hydroxide solution evenly, and sonicate at 70-80℃ for 20-30 min. After washing and drying, pretreated spandex is obtained. Adjust the pH of Tris-HCl buffer to 8.5, add dopamine hydrochloride and stir evenly to obtain dopamine hydrochloride solution. Add the pretreated spandex and stir for 22-24 h. After drying, modified spandex is obtained.

[0026] Step 2: Mix 3-aminopropyltriethoxysilane and ethanol aqueous solution evenly, add boron nitride, mica and modified spandex and mix evenly, heat to 70-80℃ and react for 4-6 hours, add epoxidized sericin and continue to react for 4-6 hours, after washing, filtering and drying, the complex is obtained;

[0027] Step 3: The composite is melt-spun using a screw extruder to obtain cool-feeling fibers.

[0028] Furthermore, in step one, the mass ratio of spandex chips to sodium hydroxide solution is 1:(5-10), the concentration of sodium hydroxide solution is 1-2 mol / L, the concentration of Tris-HCl buffer is 0.01 mol / L, and the concentration of dopamine hydrochloride solution is 3-6 g / L.

[0029] Furthermore, the concentration of the ethanol aqueous solution is 90–95 wt%.

[0030] Furthermore, the cooling fiber comprises the following weight components: 80-100 parts modified spandex, 2-6 parts boron nitride, 3-8 parts mica, 4-6 parts 3-aminopropyltriethoxysilane, 120-150 parts aqueous ethanol solution, and 5-10 parts epoxidized sericin.

[0031] In the above technical solution, the surface of spandex chips is initially corroded and roughened by sodium hydroxide solution to obtain pretreated spandex. Utilizing the strong adhesion of dopamine, a stable polydopamine coating is formed on the surface of the pretreated spandex, introducing a large number of active groups such as amino and hydroxyl groups. Boron nitride and mica compound powder is used as a cooling modifier, and an aminosilane coupling agent is used for surface modification to introduce amino groups, which can react with the modified spandex and also undergo a ring-opening reaction with epoxidized sericin to obtain a composite. The composite is melt-spun to obtain a cooling fiber with excellent cooling properties, durability, and comfort, suitable for various textiles and clothing products.

[0032] Furthermore, the preparation method of the epoxidized sericin is as follows: a sericin solution with a concentration of 5-6 wt% is mixed evenly with epichlorohydrin, tetrabutylammonium bromide is added, the temperature is raised to 40-50℃, the reaction is carried out for 1-2 hours, sodium hydroxide solution is added to adjust the pH of the system to 8-9, and the epoxidized sericin is obtained by vacuum distillation.

[0033] Furthermore, the epoxidized sericin comprises the following components by weight: 10-20 parts sericin solution, 0.5-1.0 parts epichlorohydrin, and 0.1-0.3 parts tetrabutylammonium bromide.

[0034] Furthermore, the screw extruder is a single-screw extruder, and the temperatures of each zone of the screw are: 140-160℃ in the feeding section, 180-200℃ in the compression section, and 200-210℃ in the metering section.

[0035] Furthermore, the spinning process conditions are: spinning temperature 210-230℃, heat setting temperature 100-110℃, and draw ratio 1.8-2.4.

[0036] Furthermore, the denim fabric has a twill weave structure of two up, one down, and one left.

[0037] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0038] 1. This invention discloses a denim fabric made of cellulose acetate and its preparation process. The process involves pre-treating the surface of spandex chips by corrosion with sodium hydroxide solution to obtain pre-treated spandex. Utilizing the strong adhesion of dopamine, a stable polydopamine coating is formed on the surface of the pre-treated spandex, introducing a large number of active groups such as amino and hydroxyl groups. This improves the compatibility and reactivity of the modifier with the spandex, facilitating the formation of subsequent composites. Boron nitride and mica compound powder is used as a cooling modifier. Surface modification is performed using an aminosilane coupling agent, introducing amino groups that can react with the modified spandex and undergo a ring-opening reaction with epoxidized sericin, introducing skin-friendly sericin to obtain a composite. The composite is then melt-spun to obtain a cooling fiber with excellent cooling properties, durability, and comfort, thus achieving a denim fabric with coolness, excellent elasticity, moisture absorption, and softness.

[0039] 2. The present invention relates to an acetate fiber woven denim fabric and its preparation process, which, by blending acetate fiber, cooling fiber and cotton fiber, can not only give full play to the advantages of each fiber, such as the antibacterial properties and durability of modified acetate fiber, the heat dissipation properties of cooling fiber, and the comfort and moisture absorption and breathability of cotton fiber, but also compensate for each other's shortcomings and jointly improve the overall performance of the fabric, thus achieving a combination of functionality and comfort. Detailed Implementation

[0040] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0041] In this embodiment, the cellulose acetate (cellulose diacetate) is sourced from Wuhan Lanabai Pharmaceutical Chemical Co., Ltd.; the cotton fiber is grade 1 cotton fiber sourced from Hebei Kexu Building Materials Co., Ltd.; the spandex chips are polyether-type TPU, grade 1580, sourced from Ningbo Aoke Polymer New Materials Co., Ltd.; the boron nitride has a particle size of 20-45μm and is sourced from Zhengzhou Jiajie Chemical Products Co., Ltd.; the mica has a particle size of 1250 mesh and is sourced from Chuzhou Baota Sericite Mining Co., Ltd.; the sericin has a product number of TK-0078 and is sourced from Shaanxi Taike Biotechnology Co., Ltd.; and the bamboo fiber is premium grade, with a fiber length of 10mm, sourced from Tongling Hongqing Hemp Industry Co., Ltd.

[0042] In the following examples and comparative examples, 1 part equals 10g.

[0043] Example 1: A process for preparing acetate fiber denim fabric, comprising the following steps:

[0044] Step S1: Blend 50 parts of acetate fiber, 50 parts of cooling fiber and 100 parts of cotton fiber to obtain warp yarn;

[0045] Step S2: Blend 50 parts of cooling fiber, 100 parts of cotton fiber and 25 parts of bamboo fiber to obtain weft yarn;

[0046] Step S3: Weave the warp and weft yarns to obtain the greige fabric. Then, sequentially perform greige fabric turning, singeing, desizing, stretching, and pre-shrinking to obtain denim fabric.

[0047] The preparation method of cellulose acetate is as follows:

[0048] Step (1): Under nitrogen protection, 50 parts of cellulose acetate, 600 parts of N,N-dimethylacetamide, and 40 parts of triethylamine were mixed evenly. The system temperature was adjusted to -10℃. A mixed solution of 40 parts of methacryloyl chloride and 240 parts of N,N-dimethylacetamide was added dropwise over 1 hour. The temperature was then raised to 20℃ and the reaction was carried out for 22 hours. After filtration, washing, and drying, cellulose acetate containing double bonds was obtained.

[0049] Step (2): Mix 50 parts of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 40 parts of 2-chloro-4,6-dimethoxy-1,3,5-triazine and 250 parts of anhydrous N,N-dimethylformamide evenly, react in an ice bath for 1 hour, adjust the pH of the system to 7.3, add 20 parts of methacrylamide and mix evenly, react in an ice bath for 3 hours, and obtain the antibacterial agent after rotary evaporation;

[0050] Step (3): Under nitrogen protection, 50 parts of double-bonded cellulose acetate, 50 parts of antibacterial agent and 200 parts of deionized water are mixed evenly, heated to 70°C, and a mixed solution of 1.5 parts of potassium persulfate and 450 parts of deionized water is added dropwise over 1 hour. The reaction is carried out over 6 hours. After filtration, washing and drying, modified cellulose acetate is obtained.

[0051] Step (4): Mix 50 parts of modified cellulose acetate and 100 parts of dichloromethane evenly, and use dry spinning method to obtain cellulose acetate;

[0052] The preparation method of cooling fiber is as follows:

[0053] Step 1: Mix 80 parts of spandex slices and 400 parts of 1 mol / L sodium hydroxide solution evenly, sonicate at 70℃ for 20 min, and after washing and drying, obtain pretreated spandex; adjust the pH of 0.01 mol / L Tris-HCl buffer to 8.5, add dopamine hydrochloride and stir evenly to obtain a 3 g / L dopamine hydrochloride solution, add 80 parts of pretreated spandex, stir for 22 h, and after drying, obtain modified spandex;

[0054] Step 2: Mix 4 parts of 3-aminopropyltriethoxysilane and 120 parts of 90wt% ethanol aqueous solution evenly, add 2 parts of boron nitride, 3 parts of mica and 80 parts of modified spandex and mix evenly, heat to 70℃ and react for 4 hours, add 5 parts of epoxidized sericin and continue to react for 4 hours, after washing, filtering and drying, the complex is obtained.

[0055] Step 3: The composite is melt-spun through a screw extruder (the temperature of each zone of the screw is: 140℃ in the feeding section, 180℃ in the compression section, 200℃ in the metering section, 210℃ in the spinning temperature, 100℃ in the heat setting temperature, and 1.8 in the draw ratio) to obtain cool-feeling fibers.

[0056] The preparation method of epoxidized sericin is as follows: 10 parts of 5wt% sericin solution and 0.5 parts of epichlorohydrin are mixed evenly, 0.1 parts of tetrabutylammonium bromide are added, the temperature is raised to 40℃, the reaction is carried out for 1 hour, sodium hydroxide solution is added to adjust the pH of the system to 8, and epoxidized sericin is obtained by vacuum distillation.

[0057] Example 2: A process for preparing acetate fiber denim fabric, comprising the following steps:

[0058] Step S1: Blend 50 parts of acetate fiber, 75 parts of cooling fiber and 125 parts of cotton fiber to obtain warp yarn;

[0059] Step S2: Blend 50 parts of cooling fiber, 125 parts of cotton fiber and 40 parts of bamboo fiber to obtain weft yarn;

[0060] Step S3: Weave the warp and weft yarns to obtain the greige fabric. Then, sequentially perform greige fabric turning, singeing, desizing, stretching, and pre-shrinking to obtain denim fabric.

[0061] The preparation method of cellulose acetate is as follows:

[0062] Step (1): Under nitrogen protection, 50 parts of cellulose acetate, 650 parts of N,N-dimethylacetamide, and 45 parts of triethylamine were mixed evenly. The system temperature was adjusted to -8℃. A mixed solution of 45 parts of methacryloyl chloride and 310 parts of N,N-dimethylacetamide was added dropwise over 1.5 hours. The temperature was then raised to 25℃ and the reaction was allowed to proceed for 22 hours. After filtration, washing, and drying, cellulose acetate containing double bonds was obtained.

[0063] Step (2): Mix 60 parts of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 54 parts of 2-chloro-4,6-dimethoxy-1,3,5-triazine and 360 parts of anhydrous N,N-dimethylformamide evenly, react in an ice bath for 1.5 h, adjust the pH of the system to 7.4, add 27 parts of methacrylamide and mix evenly, react in an ice bath for 4 h, and obtain the antibacterial agent after rotary evaporation;

[0064] Step (3): Under nitrogen protection, 50 parts of cellulose acetate containing double bonds, 60 parts of antibacterial agent and 250 parts of deionized water are mixed evenly, heated to 75°C, and a mixed solution of 2 parts of potassium persulfate and 700 parts of deionized water is added dropwise over 1.5 hours. After 7 hours of reaction, the modified cellulose acetate is obtained by filtration, washing and drying.

[0065] Step (4): Mix 50 parts of modified cellulose acetate and 150 parts of dichloromethane evenly, and use dry spinning method to obtain cellulose acetate;

[0066] The preparation method of cooling fiber is as follows:

[0067] Step 1: Mix 90 parts of spandex chips and 720 parts of 1.5 mol / L sodium hydroxide solution evenly, sonicate at 75℃ for 25 min, and after washing and drying, obtain pretreated spandex; adjust the pH of 0.01 mol / L Tris-HCl buffer to 8.5, add dopamine hydrochloride and stir evenly to obtain a 5 g / L dopamine hydrochloride solution, add 90 parts of pretreated spandex, stir for 23 h, and after drying, obtain modified spandex;

[0068] Step 2: Mix 5 parts of 3-aminopropyltriethoxysilane and 130 parts of 95wt% ethanol aqueous solution evenly, add 4 parts of boron nitride, 5 parts of mica and 90 parts of modified spandex and mix evenly, heat to 75℃ and react for 5 hours, add 8 parts of epoxidized sericin and continue to react for 5 hours, after washing, filtering and drying, the complex is obtained.

[0069] Step 3: The composite is melt-spun through a screw extruder (the temperature of each zone of the screw is: 150℃ in the feeding section, 190℃ in the compression section, 210℃ in the metering section, 220℃ in the spinning temperature, 105℃ in the heat setting temperature, and 2.0 in the draw ratio) to obtain cool-feeling fibers.

[0070] The preparation method of epoxidized sericin is as follows: 15 parts of 5.5wt% sericin solution and 0.8 parts of epichlorohydrin are mixed evenly, 0.2 parts of tetrabutylammonium bromide are added, the temperature is raised to 45℃, the reaction is carried out for 1.5h, sodium hydroxide solution is added to adjust the pH of the system to 8.5, and epoxidized sericin is obtained by vacuum distillation.

[0071] Example 3: A process for preparing acetate fiber denim fabric, comprising the following steps:

[0072] Step S1: Blend 50 parts of acetate fiber, 100 parts of cooling fiber and 150 parts of cotton fiber to obtain warp yarn;

[0073] Step S2: Blend 50 parts of cooling fiber, 150 parts of cotton fiber and 50 parts of bamboo fiber to obtain weft yarn;

[0074] Step S3: Weave the warp and weft yarns to obtain the greige fabric. Then, sequentially perform greige fabric turning, singeing, desizing, stretching, and pre-shrinking to obtain denim fabric.

[0075] The preparation method of cellulose acetate is as follows:

[0076] Step (1): Under nitrogen protection, 50 parts of cellulose acetate, 750 parts of N,N-dimethylacetamide, and 50 parts of triethylamine were mixed evenly. The system temperature was adjusted to -5℃. A mixed solution of 50 parts of methacryloyl chloride and 400 parts of N,N-dimethylacetamide was added dropwise over 2 hours. The temperature was then raised to 30℃ and the reaction was carried out for 24 hours. After filtration, washing, and drying, cellulose acetate containing double bonds was obtained.

[0077] Step (2): Mix 75 parts of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 75 parts of 2-chloro-4,6-dimethoxy-1,3,5-triazine and 525 parts of anhydrous N,N-dimethylformamide evenly, react in an ice bath for 2 hours, adjust the pH of the system to 7.5, add 37.5 parts of methacrylamide and mix evenly, react in an ice bath for 5 hours, and obtain the antibacterial agent after rotary evaporation;

[0078] Step (3): Under nitrogen protection, 50 parts of double-bonded cellulose acetate, 75 parts of antibacterial agent and 300 parts of deionized water are mixed evenly, heated to 80°C, and a mixed solution of 2.5 parts of potassium persulfate and 1000 parts of deionized water is added dropwise over 2 hours. The reaction is carried out for 8 hours. After filtration, washing and drying, modified cellulose acetate is obtained.

[0079] Step (4): Mix 50 parts of modified cellulose acetate and 200 parts of dichloromethane evenly, and use dry spinning method to obtain cellulose acetate;

[0080] The preparation method of cooling fiber is as follows:

[0081] Step 1: Mix 100 parts of spandex chips and 1000 parts of 2 mol / L sodium hydroxide solution evenly, and sonicate at 80℃ for 30 min. After washing and drying, pretreated spandex is obtained. Adjust the pH of 0.01 mol / L Tris-HCl buffer to 8.5, add dopamine hydrochloride and stir evenly to obtain a 6 g / L dopamine hydrochloride solution. Add the pretreated spandex, stir for 24 h, and dry to obtain modified spandex.

[0082] Step 2: Mix 6 parts of 3-aminopropyltriethoxysilane and 150 parts of 95wt% ethanol aqueous solution evenly, add 6 parts of boron nitride, 8 parts of mica and 100 parts of modified spandex and mix evenly, heat to 80℃ and react for 6 hours, add 10 parts of epoxidized sericin and continue to react for 6 hours, after washing, filtering and drying, the complex is obtained.

[0083] Step 3: The composite is melt-spun through a screw extruder (the screw temperature in each zone is: 160℃ for the feeding section, 200℃ for the compression section, 210℃ for the metering section, 230℃ for the spinning temperature, 110℃ for the heat setting temperature, and 2.4 for the draw ratio) to obtain cool-feeling fibers.

[0084] The preparation method of epoxidized sericin is as follows: 20 parts of sericin solution with a concentration of 6wt% and 1 part of epichlorohydrin are mixed evenly, 0.3 parts of tetrabutylammonium bromide are added, the temperature is raised to 50℃, the reaction is carried out for 2 hours, sodium hydroxide solution is added to adjust the pH of the system to 9, and epoxidized sericin is obtained by vacuum distillation.

[0085] Comparative Example 1: A process for preparing acetate fiber denim fabric, comprising the following steps:

[0086] Compared with Example 2, in step S1 of Comparative Example 1, the mass ratio of cellulose acetate, cooling fiber and cotton fiber is 0.2:1.5:2.5, and the other steps and processes are the same as in Example 2.

[0087] Comparative Example 2: A process for preparing acetate fiber denim fabric, comprising the following processes:

[0088] The preparation method of cellulose acetate is as follows:

[0089] Step (1): Under nitrogen protection, 50 parts of cellulose acetate, 650 parts of N,N-dimethylacetamide, and 45 parts of triethylamine were mixed evenly. The system temperature was adjusted to -8℃. A mixed solution of 45 parts of methacryloyl chloride and 310 parts of N,N-dimethylacetamide was added dropwise over 1.5 hours. The temperature was then raised to 25℃ and the reaction was allowed to proceed for 22 hours. After filtration, washing, and drying, cellulose acetate containing double bonds was obtained.

[0090] Step (2): Mix 60 parts of 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 54 parts of 2-chloro-4,6-dimethoxy-1,3,5-triazine and 360 parts of anhydrous N,N-dimethylformamide evenly, react in an ice bath for 1.5 h, adjust the pH of the system to 7.4, add 27 parts of methacrylamide and mix evenly, react in an ice bath for 4 h, and obtain the antibacterial agent after rotary evaporation;

[0091] Step (3): Under nitrogen protection, 50 parts of cellulose acetate containing double bonds, 60 parts of antibacterial agent and 250 parts of deionized water are mixed evenly, heated to 75°C, and a mixed solution of 2 parts of potassium persulfate and 700 parts of deionized water is added dropwise over 1.5 hours. After 7 hours of reaction, the modified cellulose acetate is obtained by filtration, washing and drying.

[0092] Step (4): Mix 50 parts of modified cellulose acetate and 150 parts of dichloromethane evenly, and use dry spinning method to obtain cellulose acetate;

[0093] Compared with Example 2, in step (3) of Comparative Example 2, the mass ratio of double-bonded cellulose acetate to antibacterial agent is 1:0.5; other steps are the same as in Example 2.

[0094] Comparative Example 3: The cooling fiber comprises the following weight components: 90 parts spandex chips, 4 parts boron nitride, 5 parts mica, 5 parts 3-aminopropyltriethoxysilane, 130 parts ethanol aqueous solution, and 8 parts epoxidized sericin. Other steps and processes are the same as in Example 2.

[0095] Comparative Example 4: The cooling fiber comprises the following components by weight: 90 parts modified spandex, 1 part boron nitride, 5 parts 3-aminopropyltriethoxysilane, 130 parts ethanol aqueous solution, and 8 parts epoxidized sericin. Other steps and processes are the same as in Example 2.

[0096] Experiment: Denim fabrics obtained in Examples 1-3 and Comparative Examples 1-4 were used to prepare samples. Their properties were tested and the test results were recorded.

[0097] The instantaneous cooling performance was determined according to GB / T 35263-2017 "Test and Evaluation of Instantaneous Cooling Properties of Textiles". The evaluation standard is: instantaneous cooling sensation greater than or equal to 0.24 J / (cm). 2 ·s) is A; the instantaneous cooling sensation upon contact is greater than or equal to 0.15 J / (cm). 2 ·s), less than 0.24 J / (cm) 2 ·s) is B, and the instantaneous cooling sensation upon contact is less than 0.15 J / (cm). 2 •s) is C; the elastic recovery rate was determined according to FZ / T 01034-2008 "Textiles - Test Method for Tensile Elasticity of Woven Fabrics", with a stretching distance of 100 mm, a stretching rate of 100 mm / min, a pre-tension of 5 N, and repeated stretching 5 times; the moisture absorption performance was determined according to GB / T21655.1 standard, using a dropper perpendicular to the fabric at a distance of about 1 cm, dropping a drop of 0.2 mL of deionized water, and recording the time for complete diffusion of the water droplet to detect the moisture absorption performance; the antibacterial rate was determined according to AATCC 100-2012 "Evaluation Method for Antibacterial Textiles", with a sample size of 3.5 cm × 3.5 cm, sterilized at 121 °C for 15 min, placed in sterilized culture medium, and 0.6 mL of 10 4After contacting the sample with CFU / mL Staphylococcus aureus solution for 1 hour, the sample was placed in 60 mL of 0.05% sodium thiosulfate solution and shaken for 3 minutes. After shaking, the sample was diluted sequentially according to the tenfold dilution method and added dropwise to sterile culture medium. The sample was then incubated in a 37°C incubator for 18 hours and the antibacterial rate was calculated.

[0098] Test Results

[0099] Cooling sensation upon contact Elastic recovery rate / % hygroscopicity / s Antibacterial rate / % Example 1 A 95.4 0.30 99.3 Example 2 A 96.8 0.28 99.5 Example 3 A 94.7 0.31 99.4 Comparative Example 1 A 89.5 0.32 96.2 Comparative Example 2 A 92.3 0.34 95.8 Comparative Example 3 B 86.2 0.36 99.2 Comparative Example 4 C 90.6 0.35 99.0

[0100] Based on the data in the table above, the following conclusions can be clearly drawn:

[0101] 1. Compared with Examples 1-3, the antibacterial rate of the products obtained in Comparative Examples 1 and 2 decreased, indicating that reducing the amount of acetate fiber added would reduce the antibacterial rate of the fabric. It can be seen that the performance of the acetate fiber prepared by the present invention is affected by the ratio of each reagent in its preparation process. By selecting the mass ratio within the range mentioned above, the acetate fiber prepared has excellent antibacterial properties.

[0102] 2. Compared with Examples 1-3, the products obtained in Comparative Examples 3 and 4 showed a decrease in instantaneous cooling properties, elasticity, and moisture absorption. This indicates that compared with spandex chips, the modified spandex prepared by this invention can improve the compatibility and reactivity between the cooling modifier and spandex, thereby achieving better results. At the same time, the performance of the cooling fiber prepared by this invention is affected by its component ratio. By selecting the component ratio within the range described above, materials with excellent performance can be prepared.

[0103] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process method article or apparatus.

[0104] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A process for preparing acetate fiber denim fabric, characterized in that: Includes the following steps: Step S1: Blend cellulose acetate, cooling fiber and cotton fiber to obtain warp yarn; Step S2: Blend the cooling fiber, cotton fiber and bamboo fiber to obtain the weft yarn; Step S3: Weave the warp and weft yarns to obtain the greige fabric. Then, sequentially perform greige fabric turning, singeing, desizing, stretching, and pre-shrinking to obtain denim fabric. The method for preparing the cellulose acetate is as follows: Step (1): Under nitrogen protection, cellulose acetate, N,N-dimethylacetamide, and triethylamine are mixed evenly, the system temperature is adjusted to -10 to -5℃, and a mixed solution of methacryloyl chloride and N,N-dimethylacetamide is added dropwise over 1 to 2 hours. The temperature is then raised to 20 to 30℃ and the reaction is carried out for 22 to 24 hours. After filtration, washing, and drying, cellulose acetate containing double bonds is obtained. Step (2): Mix 4-(3,5-dioxo-1,2,4-triazolidine-4-yl)benzoic acid, 2-chloro-4,6-dimethoxy-1,3,5-triazine and anhydrous N,N-dimethylformamide evenly, react in an ice bath for 1-2 hours, adjust the pH of the system to 7.3-7.5, add methacrylamide and mix evenly, react in an ice bath for 3-5 hours, and obtain the antibacterial agent after rotary evaporation; Step (3): Under nitrogen protection, mix cellulose acetate containing double bonds, antibacterial agent and deionized water evenly, heat to 70-80℃, add potassium persulfate and deionized water solution dropwise over 1-2 hours, react for 6-8 hours, filter, wash and dry to obtain modified cellulose acetate. Step (4): Mix the modified cellulose acetate and dichloromethane evenly, and use dry spinning method to obtain cellulose acetate.

2. The preparation process of acetate fiber denim fabric according to claim 1, characterized in that: The mass ratio of the acetate fiber, the cooling fiber and the cotton fiber is 1:(1-2):(2-3).

3. The preparation process of acetate fiber denim fabric according to claim 1, characterized in that: The mass ratio of the cooling fiber, cotton fiber and bamboo fiber is 1:(2-3):(0.5-1.0).

4. The preparation process of acetate fiber denim fabric according to claim 1, characterized in that: In step (3), the mass ratio of double-bonded cellulose acetate, antibacterial agent and deionized water is 1:(1.0-1.5):(4-6); the mass of potassium persulfate is 3-5% of the mass of double-bonded cellulose acetate, and the mass ratio of potassium persulfate and deionized water is 1:(300-400).

5. The preparation process of acetate fiber denim fabric according to claim 1, characterized in that: The method for preparing the cooling fiber is as follows: Step 1: Mix spandex slices and sodium hydroxide solution evenly, and sonicate at 70-80℃ for 20-30 min. After washing and drying, pretreated spandex is obtained. Adjust the pH of Tris-HCl buffer to 8.5, add dopamine hydrochloride and stir evenly to obtain dopamine hydrochloride solution. Add the pretreated spandex and stir for 22-24 h. After drying, modified spandex is obtained. Step 2: Mix 3-aminopropyltriethoxysilane and ethanol evenly, add boron nitride, mica and modified spandex and mix evenly, heat to 70-80℃ and react for 4-6 hours, add epoxidized sericin and continue to react for 4-6 hours, after washing, filtering and drying, the complex is obtained; Step 3: The composite is melt-spun using a screw extruder to obtain cool-feeling fibers.

6. The preparation process of acetate fiber denim fabric according to claim 5, characterized in that: The cooling fiber comprises the following components by weight: 80-100 parts modified spandex, 2-6 parts boron nitride, 3-8 parts mica, 4-6 parts 3-aminopropyltriethoxysilane, 120-150 parts ethanol, and 5-10 parts epoxidized sericin.

7. The preparation process of acetate fiber denim fabric according to claim 6, characterized in that: The preparation method of the epoxidized sericin is as follows: a sericin solution with a concentration of 5-6 wt% is mixed evenly with epichlorohydrin, tetrabutylammonium bromide is added, the temperature is raised to 40-50℃, the reaction is carried out for 1-2 hours, sodium hydroxide solution is added to adjust the pH of the system to 8-9, and the epoxidized sericin is obtained by vacuum distillation.

8. The preparation process of acetate fiber denim fabric according to claim 7, characterized in that: The epoxidized sericin comprises the following components by weight: 10-20 parts sericin solution, 0.5-1.0 parts epichlorohydrin, and 0.1-0.3 parts tetrabutylammonium bromide.

9. An acetate fiber textile denim fabric prepared according to any one of claims 1 to 8.